Trifluoroacetic acid → (R)-5-(1-methanesulfonyl-1,2,3,6-tetrahydro-pyridin-4-yl)-2-piperidin-4-yl-2,3-dihydro-furo[2,3-c]pyridine

HRID 872200ノート

反応式

HRID 872200 の反応式
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:20][CH2:19][CH:18]([C@@H:21]2[O:39][C:24]3=[CH:25][N:26]=[C:27]([C:29]4[CH2:30][CH2:31][N:32]([S:35]([CH3:38])(=[O:37])=[O:36])[CH2:33][CH:34]=4)[CH:28]=[C:23]3[CH2:22]2)[CH2:17][CH2:16]1)=O)(C)(C)C>ClCCl.[OH-].[Na+].C([O-])([O-])=O.[Na+].[Na+]>[CH3:38][S:35]([N:32]1[CH2:31][CH:30]=[C:29]([C:27]2[CH:28]=[C:23]3[CH2:22][C@H:21]([CH:18]4[CH2:19][CH2:20][NH:15][CH2:16][CH2:17]4)[O:39][C:24]3=[CH:25][N:26]=2)[CH2:34][CH2:33]1)(=[O:36])=[O:37]

参加物

6

反応物 2

HCID 6422Trifluoroacetic acidHCID 71208290HCID 71208290、化合物

生成物 1

HCID 71208337(R)-5-(1-methanesulfonyl-1,2,3,6-tetrahydro-pyridin-4-yl)-2-piperidin-4-yl-2,3-dihydro-furo[2,3-c]pyridine

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒2 回HCID 10340Sodium Carbonate溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

Trifluoroacetic acid (2 mL) is added to a solution of (R)-4-[5-(1-methanesulfonyl-1,2,3,6-tetrahydro-pyridin-4-yl)-2,3-dihydro-furo[2,3-c]pyridin-2-yl]-piperidine-1-carboxylic acid tert-butyl ester (1.0 g) in dichloromethane (10 mL) at room temperature. The solution is stirred at room temperature overnight and then diluted with dichloromethane, 2 N aqueous NaOH solution, and saturated aqueous Na2CO3 solution. The resulting mixture is vigorously stirred for 20 min and then extracted with dichloromethane. The combined extract is dried (Na2SO4) and concentrated to give the title compound. Mass spectrum (ESI+): m/z=364 [M+H]+.

後処理

  1. stirringThe resulting mixture is vigorously stirred for 20 min
  2. extractionextracted with dichloromethane
  3. extractionThe combined extract
  4. dry with materialis dried (Na2SO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-8a155cdebad54860ba055472dd3ebcb6
出典データセット
uspto-grants-2015_03
特許番号
US08975277B2

反応ノート

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